# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_r
_database_code_depnum_ccdc_archive 'CCDC 912390'
_audit_update_record             
;
2016-03-17 deposited with the CCDC.
2016-09-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C64 H46 N6 S2'
_chemical_formula_weight         963.19

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)/c  '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   15.423(5)
_cell_length_b                   41.104(5)
_cell_length_c                   9.126(5)
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 120.433(5)
_cell_angle_gamma                90.000(5)
_cell_volume                     4988(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    327(2)
_cell_measurement_reflns_used    4059
_cell_measurement_theta_min      2.45
_cell_measurement_theta_max      20.88

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2016
_exptl_absorpt_coefficient_mu    0.156
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.9547
_exptl_absorpt_correction_T_max  0.9695
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      327(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            35585
_diffrn_reflns_av_R_equivalents  0.0619
_diffrn_reflns_av_sigmaI/netI    0.0614
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         0.99
_diffrn_reflns_theta_max         25.00
_reflns_number_total             8781
_reflns_number_gt                5133
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1497P)²+4.8152P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8781
_refine_ls_number_parameters     649
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1083
_refine_ls_R_factor_gt           0.0549
_refine_ls_wR_factor_ref         0.2163
_refine_ls_wR_factor_gt          0.1573
_refine_ls_goodness_of_fit_ref   0.780
_refine_ls_restrained_S_all      0.780
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.36090(7) 0.21982(2) 0.43040(12) 0.0553(3) Uani 1 1 d . . .
S2 S 0.74550(7) 0.03964(2) 0.38054(12) 0.0571(3) Uani 1 1 d . . .
N4 N 1.0372(2) -0.00016(7) 0.2671(4) 0.0506(7) Uani 1 1 d . . .
N6 N 0.5623(2) 0.04451(8) 0.3593(4) 0.0580(8) Uani 1 1 d . . .
N3 N 0.2174(2) 0.19299(8) 0.1311(3) 0.0535(8) Uani 1 1 d . . .
C27 C 0.2298(3) 0.19161(8) -0.0125(4) 0.0473(8) Uani 1 1 d . . .
N1 N 0.6896(2) 0.22919(8) 1.0590(4) 0.0535(8) Uani 1 1 d . . .
C38 C 1.0152(3) 0.02670(9) 0.3247(4) 0.0480(8) Uani 1 1 d . . .
C12 C 0.6264(2) 0.25022(9) 0.9383(4) 0.0479(8) Uani 1 1 d . . .
C21 C 0.1256(3) 0.20317(9) 0.1194(4) 0.0490(9) Uani 1 1 d . . .
C64 C 0.5878(3) 0.04704(9) 0.5324(5) 0.0524(9) Uani 1 1 d . . .
C17 C 0.4493(2) 0.19435(8) 0.5827(4) 0.0447(8) Uani 1 1 d . . .
C57 C 0.4850(3) 0.06411(9) 0.2305(4) 0.0536(9) Uani 1 1 d . . .
C46 C 0.8584(2) 0.00471(8) 0.2756(4) 0.0454(8) Uani 1 1 d . . .
C16 C 0.5307(2) 0.20677(9) 0.7476(4) 0.0462(8) Uani 1 1 d . . .
C44 C 0.9713(3) -0.02505(9) 0.2152(4) 0.0502(9) Uani 1 1 d . . .
C6 C 0.7457(3) 0.17510(10) 1.1626(4) 0.0526(9) Uani 1 1 d . . .
C48 C 0.7634(3) 0.00764(8) 0.2765(4) 0.0465(8) Uani 1 1 d . . .
C13 C 0.6742(3) 0.19722(9) 1.0265(4) 0.0484(9) Uani 1 1 d . . .
C43 C 1.0006(3) -0.05444(9) 0.1572(5) 0.0526(9) Uani 1 1 d . . .
C20 C 0.3011(3) 0.18771(9) 0.2946(4) 0.0486(9) Uani 1 1 d . . .
C37 C 1.0908(3) 0.05341(9) 0.3866(5) 0.0520(9) Uani 1 1 d . . .
C47 C 0.9275(3) 0.02975(9) 0.3310(4) 0.0504(9) Uani 1 1 d . . .
H47 H 0.9152 0.0488 0.3728 0.060 Uiso 1 1 calc R . .
C45 C 0.8820(3) -0.02337(9) 0.2169(4) 0.0512(9) Uani 1 1 d . . .
H45 H 0.8379 -0.0409 0.1789 0.061 Uiso 1 1 calc R . .
C18 C 0.4326(3) 0.16308(9) 0.5269(5) 0.0580(10) Uani 1 1 d . . .
H18 H 0.4731 0.1458 0.5907 0.070 Uiso 1 1 calc R . .
C14 C 0.5955(3) 0.18538(9) 0.8739(4) 0.0510(9) Uani 1 1 d . . .
H14 H 0.5862 0.1631 0.8563 0.061 Uiso 1 1 calc R . .
C51 C 0.6246(3) 0.02656(10) 0.3164(4) 0.0521(9) Uani 1 1 d . . .
C19 C 0.3479(3) 0.15935(10) 0.3627(5) 0.0595(10) Uani 1 1 d . . .
H19 H 0.3267 0.1394 0.3074 0.071 Uiso 1 1 calc R . .
C15 C 0.5470(3) 0.23987(9) 0.7820(4) 0.0505(9) Uani 1 1 d . . .
H15 H 0.5051 0.2550 0.7014 0.061 Uiso 1 1 calc R . .
C49 C 0.6802(3) -0.01144(10) 0.1995(5) 0.0575(10) Uani 1 1 d . . .
H49 H 0.6758 -0.0299 0.1369 0.069 Uiso 1 1 calc R . .
C59 C 0.5608(3) 0.07377(10) 0.5917(5) 0.0629(10) Uani 1 1 d . . .
H59 H 0.5257 0.0909 0.5186 0.076 Uiso 1 1 calc R . .
C50 C 0.6016(3) -0.00087(10) 0.2230(5) 0.0596(10) Uani 1 1 d . . .
H50 H 0.5403 -0.0116 0.1789 0.072 Uiso 1 1 calc R . .
C7 C 0.6464(3) 0.28525(10) 0.9812(5) 0.0549(9) Uani 1 1 d . . .
C32 C 0.3245(3) 0.19271(10) 0.0068(5) 0.0594(10) Uani 1 1 d . . .
H32 H 0.3809 0.1945 0.1148 0.071 Uiso 1 1 calc R . .
C28 C 0.1471(3) 0.18849(10) -0.1754(5) 0.0618(10) Uani 1 1 d . . .
H28 H 0.0828 0.1872 -0.1908 0.074 Uiso 1 1 calc R . .
C22 C 0.0864(3) 0.18564(11) 0.1991(5) 0.0622(11) Uani 1 1 d . . .
H22 H 0.1198 0.1672 0.2608 0.075 Uiso 1 1 calc R . .
C63 C 0.6418(3) 0.02213(11) 0.6437(5) 0.0666(11) Uani 1 1 d . . .
H63 H 0.6605 0.0040 0.6054 0.080 Uiso 1 1 calc R . .
C1 C 0.8038(3) 0.18578(11) 1.3294(5) 0.0591(10) Uani 1 1 d . . .
H1 H 0.7986 0.2072 1.3563 0.071 Uiso 1 1 calc R . .
C8 C 0.7198(3) 0.29517(12) 1.1418(6) 0.0722(12) Uani 1 1 d . . .
H8 H 0.7565 0.2798 1.2252 0.087 Uiso 1 1 calc R . .
C62 C 0.6679(3) 0.02450(12) 0.8134(5) 0.0730(12) Uani 1 1 d . . .
H62 H 0.7050 0.0079 0.8886 0.088 Uiso 1 1 calc R . .
N5 N 0.9479(4) -0.08253(10) 0.1327(7) 0.1053(15) Uani 1 1 d . . .
N2 N 0.5901(3) 0.30721(9) 0.8568(6) 0.0834(11) Uani 1 1 d . . .
C31 C 0.3355(4) 0.19112(11) -0.1352(6) 0.0738(12) Uani 1 1 d . . .
H31 H 0.3994 0.1918 -0.1215 0.089 Uiso 1 1 calc R . .
C56 C 0.3908(3) 0.06449(11) 0.2132(6) 0.0699(12) Uani 1 1 d . . .
H56 H 0.3777 0.0514 0.2830 0.084 Uiso 1 1 calc R . .
C36 C 1.0742(3) 0.08062(10) 0.4485(6) 0.0743(13) Uani 1 1 d . . .
H36 H 1.0144 0.0831 0.4490 0.089 Uiso 1 1 calc R . .
C60 C 0.5860(4) 0.07509(11) 0.7603(5) 0.0735(12) Uani 1 1 d . . .
H60 H 0.5659 0.0929 0.7987 0.088 Uiso 1 1 calc R . .
C39 C 1.0778(3) -0.05376(12) 0.1242(6) 0.0795(14) Uani 1 1 d . . .
H39 H 1.1142 -0.0347 0.1417 0.095 Uiso 1 1 calc R . .
C26 C 0.0762(3) 0.23076(11) 0.0295(6) 0.0727(12) Uani 1 1 d . . .
H26 H 0.1031 0.2432 -0.0230 0.087 Uiso 1 1 calc R . .
C5 C 0.7560(3) 0.14353(10) 1.1262(5) 0.0714(12) Uani 1 1 d . . .
H5 H 0.7178 0.1358 1.0154 0.086 Uiso 1 1 calc R . .
C52 C 0.5022(4) 0.08239(12) 0.1217(6) 0.0799(13) Uani 1 1 d . . .
H52 H 0.5650 0.0821 0.1305 0.096 Uiso 1 1 calc R . .
C61 C 0.6399(4) 0.05080(12) 0.8711(5) 0.0739(12) Uani 1 1 d . . .
H61 H 0.6574 0.0521 0.9846 0.089 Uiso 1 1 calc R . .
C23 C -0.0030(3) 0.19510(13) 0.1891(5) 0.0751(13) Uani 1 1 d . . .
H23 H -0.0294 0.1830 0.2434 0.090 Uiso 1 1 calc R . .
C2 C 0.8689(3) 0.16492(14) 1.4553(5) 0.0763(13) Uani 1 1 d . . .
H2 H 0.9068 0.1722 1.5668 0.092 Uiso 1 1 calc R . .
C25 C -0.0134(4) 0.23982(14) 0.0178(7) 0.0880(15) Uani 1 1 d . . .
H25 H -0.0476 0.2580 -0.0460 0.106 Uiso 1 1 calc R . .
C9 C 0.7384(4) 0.32754(15) 1.1785(8) 0.0947(17) Uani 1 1 d . . .
H9 H 0.7882 0.3342 1.2860 0.114 Uiso 1 1 calc R . .
C29 C 0.1599(4) 0.18737(11) -0.3137(5) 0.0751(13) Uani 1 1 d . . .
H29 H 0.1039 0.1857 -0.4221 0.090 Uiso 1 1 calc R . .
C42 C 0.9756(4) -0.10974(13) 0.0777(8) 0.1044(19) Uani 1 1 d . . .
H42 H 0.9418 -0.1292 0.0658 0.125 Uiso 1 1 calc R . .
C55 C 0.3161(4) 0.08408(13) 0.0932(7) 0.0868(16) Uani 1 1 d . . .
H55 H 0.2534 0.0848 0.0848 0.104 Uiso 1 1 calc R . .
C30 C 0.2533(4) 0.18859(11) -0.2947(6) 0.0768(13) Uani 1 1 d . . .
H30 H 0.2611 0.1877 -0.3892 0.092 Uiso 1 1 calc R . .
C24 C -0.0523(3) 0.22252(14) 0.0982(6) 0.0796(14) Uani 1 1 d . . .
H24 H -0.1117 0.2292 0.0919 0.096 Uiso 1 1 calc R . .
C40 C 1.1021(4) -0.08120(14) 0.0648(7) 0.0947(17) Uani 1 1 d . . .
H40 H 1.1542 -0.0805 0.0416 0.114 Uiso 1 1 calc R . .
C58 C 1.1792(4) 0.05019(12) 0.3865(7) 0.0884(15) Uani 1 1 d . . .
H58 H 1.1922 0.0316 0.3427 0.106 Uiso 1 1 calc R . .
C41 C 1.0497(4) -0.10925(12) 0.0406(7) 0.0848(15) Uani 1 1 d . . .
H41 H 1.0648 -0.1278 -0.0009 0.102 Uiso 1 1 calc R . .
C35 C 1.1426(4) 0.10441(13) 0.5097(8) 0.0984(17) Uani 1 1 d . . .
H35 H 1.1284 0.1230 0.5516 0.118 Uiso 1 1 calc R . .
C11 C 0.6105(4) 0.33933(12) 0.8979(9) 0.0997(18) Uani 1 1 d . . .
H11 H 0.5735 0.3548 0.8151 0.120 Uiso 1 1 calc R . .
C3 C 0.8778(4) 0.13362(15) 1.4168(7) 0.0924(16) Uani 1 1 d . . .
H3 H 0.9212 0.1193 1.5012 0.111 Uiso 1 1 calc R . .
C53 C 0.4256(5) 0.10111(14) -0.0008(7) 0.1016(18) Uani 1 1 d . . .
H53 H 0.4368 0.1131 -0.0761 0.122 Uiso 1 1 calc R . .
C54 C 0.3339(5) 0.10242(14) -0.0135(6) 0.0989(19) Uani 1 1 d . . .
H54 H 0.2836 0.1157 -0.0944 0.119 Uiso 1 1 calc R . .
C33 C 1.2494(4) 0.07543(16) 0.4535(8) 0.1059(19) Uani 1 1 d . . .
H33 H 1.3103 0.0733 0.4563 0.127 Uiso 1 1 calc R . .
C10 C 0.6836(5) 0.34987(14) 1.0564(10) 0.0988(19) Uani 1 1 d . . .
H10 H 0.6951 0.3720 1.0795 0.119 Uiso 1 1 calc R . .
C34 C 1.2309(4) 0.10277(13) 0.5140(6) 0.0850(15) Uani 1 1 d . . .
H34 H 1.2770 0.1198 0.5568 0.102 Uiso 1 1 calc R . .
C4 C 0.8215(5) 0.12346(14) 1.2508(7) 0.1035(18) Uani 1 1 d . . .
H4 H 0.8287 0.1022 1.2234 0.124 Uiso 1 1 calc R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 C20 1.724(4) . ?
S1 C17 1.723(3) . ?
S2 C48 1.725(4) . ?
S2 C51 1.733(4) . ?
N4 C44 1.348(5) . ?
N4 C38 1.338(4) . ?
N6 C57 1.426(5) . ?
N6 C51 1.414(4) . ?
N6 C64 1.425(5) . ?
N3 C20 1.410(4) . ?
N3 C27 1.418(4) . ?
N3 C21 1.427(5) . ?
C27 C28 1.390(5) . ?
C27 C32 1.380(5) . ?
N1 C13 1.342(5) . ?
N1 C12 1.351(5) . ?
C38 C47 1.389(5) . ?
C38 C37 1.488(5) . ?
C12 C15 1.394(5) . ?
C12 C7 1.483(5) . ?
C21 C22 1.364(5) . ?
C21 C26 1.381(6) . ?
C64 C63 1.385(5) . ?
C64 C59 1.379(5) . ?
C17 C18 1.358(5) . ?
C17 C16 1.479(5) . ?
C57 C56 1.379(6) . ?
C57 C52 1.374(6) . ?
C46 C47 1.380(5) . ?
C46 C45 1.396(5) . ?
C46 C48 1.474(5) . ?
C16 C15 1.391(5) . ?
C16 C14 1.390(5) . ?
C44 C45 1.387(5) . ?
C44 C43 1.479(5) . ?
C6 C5 1.369(6) . ?
C6 C1 1.389(5) . ?
C6 C13 1.483(5) . ?
C48 C49 1.357(5) . ?
C13 C14 1.392(5) . ?
C43 N5 1.364(5) . ?
C43 C39 1.368(6) . ?
C20 C19 1.346(5) . ?
C37 C36 1.335(5) . ?
C37 C58 1.371(6) . ?
C47 H47 0.9300 . ?
C45 H45 0.9300 . ?
C18 C19 1.412(5) . ?
C18 H18 0.9300 . ?
C14 H14 0.9300 . ?
C51 C50 1.348(5) . ?
C19 H19 0.9300 . ?
C15 H15 0.9300 . ?
C49 C50 1.403(5) . ?
C49 H49 0.9300 . ?
C59 C60 1.384(6) . ?
C59 H59 0.9300 . ?
C50 H50 0.9300 . ?
C7 N2 1.364(5) . ?
C7 C8 1.384(6) . ?
C32 C31 1.392(6) . ?
C32 H32 0.9300 . ?
C28 C29 1.373(6) . ?
C28 H28 0.9300 . ?
C22 C23 1.391(6) . ?
C22 H22 0.9300 . ?
C63 C62 1.393(6) . ?
C63 H63 0.9300 . ?
C1 C2 1.376(6) . ?
C1 H1 0.9300 . ?
C8 C9 1.366(7) . ?
C8 H8 0.9300 . ?
C62 C61 1.364(6) . ?
C62 H62 0.9300 . ?
N5 C42 1.380(6) . ?
N2 C11 1.365(6) . ?
C31 C30 1.366(6) . ?
C31 H31 0.9300 . ?
C56 C55 1.378(6) . ?
C56 H56 0.9300 . ?
C36 C35 1.336(6) . ?
C36 H36 0.9300 . ?
C60 C61 1.364(6) . ?
C60 H60 0.9300 . ?
C39 C40 1.383(6) . ?
C39 H39 0.9300 . ?
C26 C25 1.382(6) . ?
C26 H26 0.9300 . ?
C5 C4 1.353(6) . ?
C5 H5 0.9300 . ?
C52 C53 1.378(7) . ?
C52 H52 0.9300 . ?
C61 H61 0.9300 . ?
C23 C24 1.377(7) . ?
C23 H23 0.9300 . ?
C2 C3 1.359(7) . ?
C2 H2 0.9300 . ?
C25 C24 1.360(7) . ?
C25 H25 0.9300 . ?
C9 C10 1.358(8) . ?
C9 H9 0.9300 . ?
C29 C30 1.362(6) . ?
C29 H29 0.9300 . ?
C42 C41 1.346(7) . ?
C42 H42 0.9300 . ?
C55 C54 1.365(8) . ?
C55 H55 0.9300 . ?
C30 H30 0.9300 . ?
C24 H24 0.9300 . ?
C40 C41 1.360(7) . ?
C40 H40 0.9300 . ?
C58 C33 1.397(7) . ?
C58 H58 0.9300 . ?
C41 H41 0.9300 . ?
C35 C34 1.344(7) . ?
C35 H35 0.9300 . ?
C11 C10 1.378(8) . ?
C11 H11 0.9300 . ?
C3 C4 1.375(7) . ?
C3 H3 0.9300 . ?
C53 C54 1.360(8) . ?
C53 H53 0.9300 . ?
C54 H54 0.9300 . ?
C33 C34 1.345(7) . ?
C33 H33 0.9300 . ?
C10 H10 0.9300 . ?
C34 H34 0.9300 . ?
C4 H4 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C20 S1 C17 91.80(17) . . ?
C48 S2 C51 91.31(18) . . ?
C44 N4 C38 117.9(3) . . ?
C57 N6 C51 117.9(3) . . ?
C57 N6 C64 121.2(3) . . ?
C51 N6 C64 120.0(3) . . ?
C20 N3 C27 119.5(3) . . ?
C20 N3 C21 117.8(3) . . ?
C27 N3 C21 122.4(3) . . ?
C28 C27 C32 118.5(3) . . ?
C28 C27 N3 120.8(3) . . ?
C32 C27 N3 120.7(3) . . ?
C13 N1 C12 118.2(3) . . ?
N4 C38 C47 122.5(3) . . ?
N4 C38 C37 116.9(3) . . ?
C47 C38 C37 120.6(3) . . ?
N1 C12 C15 122.4(3) . . ?
N1 C12 C7 116.0(3) . . ?
C15 C12 C7 121.6(3) . . ?
C22 C21 C26 119.4(4) . . ?
C22 C21 N3 119.7(3) . . ?
C26 C21 N3 120.9(3) . . ?
C63 C64 C59 119.4(3) . . ?
C63 C64 N6 119.0(3) . . ?
C59 C64 N6 121.6(3) . . ?
C18 C17 C16 127.6(3) . . ?
C18 C17 S1 110.5(3) . . ?
C16 C17 S1 121.9(3) . . ?
C56 C57 C52 119.3(4) . . ?
C56 C57 N6 119.6(4) . . ?
C52 C57 N6 121.1(4) . . ?
C47 C46 C45 117.0(3) . . ?
C47 C46 C48 121.5(3) . . ?
C45 C46 C48 121.5(3) . . ?
C15 C16 C14 117.4(3) . . ?
C15 C16 C17 122.1(3) . . ?
C14 C16 C17 120.6(3) . . ?
N4 C44 C45 122.3(3) . . ?
N4 C44 C43 115.7(3) . . ?
C45 C44 C43 122.0(3) . . ?
C5 C6 C1 118.4(4) . . ?
C5 C6 C13 120.4(3) . . ?
C1 C6 C13 121.2(4) . . ?
C49 C48 C46 129.2(3) . . ?
C49 C48 S2 110.6(3) . . ?
C46 C48 S2 120.2(3) . . ?
N1 C13 C14 122.1(3) . . ?
N1 C13 C6 116.2(3) . . ?
C14 C13 C6 121.7(3) . . ?
N5 C43 C39 119.6(4) . . ?
N5 C43 C44 119.0(4) . . ?
C39 C43 C44 121.3(4) . . ?
C19 C20 N3 127.7(3) . . ?
C19 C20 S1 111.4(3) . . ?
N3 C20 S1 120.8(3) . . ?
C36 C37 C58 119.0(4) . . ?
C36 C37 C38 119.9(4) . . ?
C58 C37 C38 121.1(4) . . ?
C46 C47 C38 120.3(3) . . ?
C46 C47 H47 119.8 . . ?
C38 C47 H47 119.8 . . ?
C44 C45 C46 119.9(3) . . ?
C44 C45 H45 120.0 . . ?
C46 C45 H45 120.0 . . ?
C17 C18 C19 113.5(3) . . ?
C17 C18 H18 123.3 . . ?
C19 C18 H18 123.3 . . ?
C13 C14 C16 120.3(3) . . ?
C13 C14 H14 119.8 . . ?
C16 C14 H14 119.8 . . ?
C50 C51 N6 127.8(4) . . ?
C50 C51 S2 111.5(3) . . ?
N6 C51 S2 120.7(3) . . ?
C20 C19 C18 112.8(3) . . ?
C20 C19 H19 123.6 . . ?
C18 C19 H19 123.6 . . ?
C16 C15 C12 119.6(3) . . ?
C16 C15 H15 120.2 . . ?
C12 C15 H15 120.2 . . ?
C48 C49 C50 114.0(3) . . ?
C48 C49 H49 123.0 . . ?
C50 C49 H49 123.0 . . ?
C64 C59 C60 119.8(4) . . ?
C64 C59 H59 120.1 . . ?
C60 C59 H59 120.1 . . ?
C51 C50 C49 112.6(4) . . ?
C51 C50 H50 123.7 . . ?
C49 C50 H50 123.7 . . ?
N2 C7 C8 121.4(4) . . ?
N2 C7 C12 117.6(3) . . ?
C8 C7 C12 121.0(4) . . ?
C27 C32 C31 120.0(4) . . ?
C27 C32 H32 120.0 . . ?
C31 C32 H32 120.0 . . ?
C27 C28 C29 120.3(4) . . ?
C27 C28 H28 119.8 . . ?
C29 C28 H28 119.8 . . ?
C21 C22 C23 120.7(4) . . ?
C21 C22 H22 119.7 . . ?
C23 C22 H22 119.7 . . ?
C64 C63 C62 119.4(4) . . ?
C64 C63 H63 120.3 . . ?
C62 C63 H63 120.3 . . ?
C2 C1 C6 120.7(4) . . ?
C2 C1 H1 119.6 . . ?
C6 C1 H1 119.6 . . ?
C7 C8 C9 120.3(5) . . ?
C7 C8 H8 119.9 . . ?
C9 C8 H8 119.9 . . ?
C61 C62 C63 121.0(4) . . ?
C61 C62 H62 119.5 . . ?
C63 C62 H62 119.5 . . ?
C43 N5 C42 118.5(4) . . ?
C7 N2 C11 116.8(5) . . ?
C30 C31 C32 120.7(4) . . ?
C30 C31 H31 119.6 . . ?
C32 C31 H31 119.6 . . ?
C57 C56 C55 120.4(5) . . ?
C57 C56 H56 119.8 . . ?
C55 C56 H56 119.8 . . ?
C37 C36 C35 120.7(4) . . ?
C37 C36 H36 119.7 . . ?
C35 C36 H36 119.7 . . ?
C61 C60 C59 121.3(4) . . ?
C61 C60 H60 119.4 . . ?
C59 C60 H60 119.4 . . ?
C43 C39 C40 120.6(5) . . ?
C43 C39 H39 119.7 . . ?
C40 C39 H39 119.7 . . ?
C21 C26 C25 119.8(4) . . ?
C21 C26 H26 120.1 . . ?
C25 C26 H26 120.1 . . ?
C6 C5 C4 120.2(4) . . ?
C6 C5 H5 119.9 . . ?
C4 C5 H5 119.9 . . ?
C53 C52 C57 119.4(5) . . ?
C53 C52 H52 120.3 . . ?
C57 C52 H52 120.3 . . ?
C60 C61 C62 119.1(4) . . ?
C60 C61 H61 120.4 . . ?
C62 C61 H61 120.4 . . ?
C24 C23 C22 119.7(4) . . ?
C24 C23 H23 120.2 . . ?
C22 C23 H23 120.2 . . ?
C3 C2 C1 120.0(4) . . ?
C3 C2 H2 120.0 . . ?
C1 C2 H2 120.0 . . ?
C24 C25 C26 121.0(5) . . ?
C24 C25 H25 119.5 . . ?
C26 C25 H25 119.5 . . ?
C8 C9 C10 119.4(5) . . ?
C8 C9 H9 120.3 . . ?
C10 C9 H9 120.3 . . ?
C30 C29 C28 121.1(4) . . ?
C30 C29 H29 119.4 . . ?
C28 C29 H29 119.4 . . ?
C41 C42 N5 122.6(5) . . ?
C41 C42 H42 118.7 . . ?
N5 C42 H42 118.7 . . ?
C54 C55 C56 120.0(5) . . ?
C54 C55 H55 120.0 . . ?
C56 C55 H55 120.0 . . ?
C29 C30 C31 119.3(4) . . ?
C29 C30 H30 120.4 . . ?
C31 C30 H30 120.4 . . ?
C23 C24 C25 119.5(4) . . ?
C23 C24 H24 120.2 . . ?
C25 C24 H24 120.2 . . ?
C41 C40 C39 119.9(5) . . ?
C41 C40 H40 120.0 . . ?
C39 C40 H40 120.0 . . ?
C37 C58 C33 118.6(5) . . ?
C37 C58 H58 120.7 . . ?
C33 C58 H58 120.7 . . ?
C42 C41 C40 118.8(4) . . ?
C42 C41 H41 120.6 . . ?
C40 C41 H41 120.6 . . ?
C36 C35 C34 123.3(5) . . ?
C36 C35 H35 118.3 . . ?
C34 C35 H35 118.3 . . ?
N2 C11 C10 123.0(5) . . ?
N2 C11 H11 118.5 . . ?
C10 C11 H11 118.5 . . ?
C2 C3 C4 118.9(5) . . ?
C2 C3 H3 120.6 . . ?
C4 C3 H3 120.6 . . ?
C54 C53 C52 121.3(5) . . ?
C54 C53 H53 119.4 . . ?
C52 C53 H53 119.4 . . ?
C55 C54 C53 119.5(5) . . ?
C55 C54 H54 120.2 . . ?
C53 C54 H54 120.2 . . ?
C34 C33 C58 121.4(5) . . ?
C34 C33 H33 119.3 . . ?
C58 C33 H33 119.3 . . ?
C9 C10 C11 119.1(5) . . ?
C9 C10 H10 120.4 . . ?
C11 C10 H10 120.4 . . ?
C33 C34 C35 116.9(5) . . ?
C33 C34 H34 121.6 . . ?
C35 C34 H34 121.6 . . ?
C5 C4 C3 121.8(5) . . ?
C5 C4 H4 119.1 . . ?
C3 C4 H4 119.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C20 N3 C27 C28 163.7(4) . . . . ?
C21 N3 C27 C28 -23.6(5) . . . . ?
C20 N3 C27 C32 -15.1(5) . . . . ?
C21 N3 C27 C32 157.7(4) . . . . ?
C44 N4 C38 C47 -0.5(5) . . . . ?
C44 N4 C38 C37 178.1(3) . . . . ?
C13 N1 C12 C15 -0.6(5) . . . . ?
C13 N1 C12 C7 179.7(3) . . . . ?
C20 N3 C21 C22 -53.0(5) . . . . ?
C27 N3 C21 C22 134.1(4) . . . . ?
C20 N3 C21 C26 126.3(4) . . . . ?
C27 N3 C21 C26 -46.5(5) . . . . ?
C57 N6 C64 C63 162.3(4) . . . . ?
C51 N6 C64 C63 -28.4(5) . . . . ?
C57 N6 C64 C59 -18.3(6) . . . . ?
C51 N6 C64 C59 150.9(4) . . . . ?
C20 S1 C17 C18 1.0(3) . . . . ?
C20 S1 C17 C16 -179.7(3) . . . . ?
C51 N6 C57 C56 137.4(4) . . . . ?
C64 N6 C57 C56 -53.1(5) . . . . ?
C51 N6 C57 C52 -41.7(5) . . . . ?
C64 N6 C57 C52 127.7(4) . . . . ?
C18 C17 C16 C15 172.2(4) . . . . ?
S1 C17 C16 C15 -7.0(5) . . . . ?
C18 C17 C16 C14 -6.7(6) . . . . ?
S1 C17 C16 C14 174.1(3) . . . . ?
C38 N4 C44 C45 1.2(5) . . . . ?
C38 N4 C44 C43 -178.4(3) . . . . ?
C47 C46 C48 C49 166.5(4) . . . . ?
C45 C46 C48 C49 -12.8(6) . . . . ?
C47 C46 C48 S2 -11.2(4) . . . . ?
C45 C46 C48 S2 169.5(3) . . . . ?
C51 S2 C48 C49 -0.3(3) . . . . ?
C51 S2 C48 C46 177.8(3) . . . . ?
C12 N1 C13 C14 -0.3(5) . . . . ?
C12 N1 C13 C6 179.8(3) . . . . ?
C5 C6 C13 N1 -160.5(4) . . . . ?
C1 C6 C13 N1 19.4(5) . . . . ?
C5 C6 C13 C14 19.6(5) . . . . ?
C1 C6 C13 C14 -160.5(4) . . . . ?
N4 C44 C43 N5 168.0(4) . . . . ?
C45 C44 C43 N5 -11.6(6) . . . . ?
N4 C44 C43 C39 -13.5(5) . . . . ?
C45 C44 C43 C39 166.9(4) . . . . ?
C27 N3 C20 C19 -73.0(5) . . . . ?
C21 N3 C20 C19 113.9(4) . . . . ?
C27 N3 C20 S1 103.1(4) . . . . ?
C21 N3 C20 S1 -70.0(4) . . . . ?
C17 S1 C20 C19 -0.9(3) . . . . ?
C17 S1 C20 N3 -177.6(3) . . . . ?
N4 C38 C37 C36 -178.8(4) . . . . ?
C47 C38 C37 C36 -0.2(5) . . . . ?
N4 C38 C37 C58 -0.9(5) . . . . ?
C47 C38 C37 C58 177.7(4) . . . . ?
C45 C46 C47 C38 1.0(5) . . . . ?
C48 C46 C47 C38 -178.3(3) . . . . ?
N4 C38 C47 C46 -0.6(5) . . . . ?
C37 C38 C47 C46 -179.1(3) . . . . ?
N4 C44 C45 C46 -0.7(5) . . . . ?
C43 C44 C45 C46 178.9(3) . . . . ?
C47 C46 C45 C44 -0.4(5) . . . . ?
C48 C46 C45 C44 178.9(3) . . . . ?
C16 C17 C18 C19 179.9(3) . . . . ?
S1 C17 C18 C19 -0.9(4) . . . . ?
N1 C13 C14 C16 1.2(5) . . . . ?
C6 C13 C14 C16 -178.9(3) . . . . ?
C15 C16 C14 C13 -1.3(5) . . . . ?
C17 C16 C14 C13 177.7(3) . . . . ?
C57 N6 C51 C50 -75.2(5) . . . . ?
C64 N6 C51 C50 115.2(4) . . . . ?
C57 N6 C51 S2 103.1(4) . . . . ?
C64 N6 C51 S2 -66.5(4) . . . . ?
C48 S2 C51 C50 0.7(3) . . . . ?
C48 S2 C51 N6 -177.8(3) . . . . ?
N3 C20 C19 C18 177.0(3) . . . . ?
S1 C20 C19 C18 0.6(4) . . . . ?
C17 C18 C19 C20 0.2(5) . . . . ?
C14 C16 C15 C12 0.4(5) . . . . ?
C17 C16 C15 C12 -178.5(3) . . . . ?
N1 C12 C15 C16 0.5(5) . . . . ?
C7 C12 C15 C16 -179.8(3) . . . . ?
C46 C48 C49 C50 -178.1(3) . . . . ?
S2 C48 C49 C50 -0.2(4) . . . . ?
C63 C64 C59 C60 -1.3(6) . . . . ?
N6 C64 C59 C60 179.3(4) . . . . ?
N6 C51 C50 C49 177.5(3) . . . . ?
S2 C51 C50 C49 -0.9(4) . . . . ?
C48 C49 C50 C51 0.7(5) . . . . ?
N1 C12 C7 N2 174.1(3) . . . . ?
C15 C12 C7 N2 -5.7(5) . . . . ?
N1 C12 C7 C8 -6.0(5) . . . . ?
C15 C12 C7 C8 174.3(4) . . . . ?
C28 C27 C32 C31 0.8(6) . . . . ?
N3 C27 C32 C31 179.6(4) . . . . ?
C32 C27 C28 C29 -1.6(6) . . . . ?
N3 C27 C28 C29 179.6(4) . . . . ?
C26 C21 C22 C23 0.7(6) . . . . ?
N3 C21 C22 C23 -179.9(3) . . . . ?
C59 C64 C63 C62 0.0(6) . . . . ?
N6 C64 C63 C62 179.4(4) . . . . ?
C5 C6 C1 C2 -1.0(6) . . . . ?
C13 C6 C1 C2 179.1(4) . . . . ?
N2 C7 C8 C9 -1.1(6) . . . . ?
C12 C7 C8 C9 179.0(4) . . . . ?
C64 C63 C62 C61 0.8(7) . . . . ?
C39 C43 N5 C42 1.1(7) . . . . ?
C44 C43 N5 C42 179.7(5) . . . . ?
C8 C7 N2 C11 0.9(6) . . . . ?
C12 C7 N2 C11 -179.1(4) . . . . ?
C27 C32 C31 C30 0.2(7) . . . . ?
C52 C57 C56 C55 -2.9(6) . . . . ?
N6 C57 C56 C55 177.9(4) . . . . ?
C58 C37 C36 C35 -0.1(7) . . . . ?
C38 C37 C36 C35 177.8(5) . . . . ?
C64 C59 C60 C61 1.9(7) . . . . ?
N5 C43 C39 C40 0.6(7) . . . . ?
C44 C43 C39 C40 -177.9(4) . . . . ?
C22 C21 C26 C25 -1.6(6) . . . . ?
N3 C21 C26 C25 179.0(4) . . . . ?
C1 C6 C5 C4 -0.1(7) . . . . ?
C13 C6 C5 C4 179.8(5) . . . . ?
C56 C57 C52 C53 1.0(7) . . . . ?
N6 C57 C52 C53 -179.8(4) . . . . ?
C59 C60 C61 C62 -1.1(7) . . . . ?
C63 C62 C61 C60 -0.3(7) . . . . ?
C21 C22 C23 C24 -0.3(6) . . . . ?
C6 C1 C2 C3 0.8(7) . . . . ?
C21 C26 C25 C24 2.1(8) . . . . ?
C7 C8 C9 C10 0.7(7) . . . . ?
C27 C28 C29 C30 1.4(7) . . . . ?
C43 N5 C42 C41 -2.9(9) . . . . ?
C57 C56 C55 C54 2.3(7) . . . . ?
C28 C29 C30 C31 -0.3(7) . . . . ?
C32 C31 C30 C29 -0.5(7) . . . . ?
C22 C23 C24 C25 0.7(7) . . . . ?
C26 C25 C24 C23 -1.7(8) . . . . ?
C43 C39 C40 C41 -0.7(8) . . . . ?
C36 C37 C58 C33 0.8(7) . . . . ?
C38 C37 C58 C33 -177.0(5) . . . . ?
N5 C42 C41 C40 2.8(9) . . . . ?
C39 C40 C41 C42 -1.0(9) . . . . ?
C37 C36 C35 C34 -0.2(9) . . . . ?
C7 N2 C11 C10 -0.4(8) . . . . ?
C1 C2 C3 C4 0.5(8) . . . . ?
C57 C52 C53 C54 1.5(8) . . . . ?
C56 C55 C54 C53 0.2(8) . . . . ?
C52 C53 C54 C55 -2.1(9) . . . . ?
C37 C58 C33 C34 -1.4(9) . . . . ?
C8 C9 C10 C11 -0.3(8) . . . . ?
N2 C11 C10 C9 0.1(9) . . . . ?
C58 C33 C34 C35 1.2(9) . . . . ?
C36 C35 C34 C33 -0.4(9) . . . . ?
C6 C5 C4 C3 1.4(9) . . . . ?
C2 C3 C4 C5 -1.7(9) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.225
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.039
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_a
_database_code_depnum_ccdc_archive 'CCDC 1465317'
_audit_update_record             
;
2016-06-07 deposited with the CCDC.
2016-09-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C31 H22 N4 S'
_chemical_formula_weight         482.59

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)/n  '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   9.148(6)
_cell_length_b                   14.095(9)
_cell_length_c                   18.970(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.977(10)
_cell_angle_gamma                90.00
_cell_volume                     2445(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    826
_cell_measurement_theta_min      2.51
_cell_measurement_theta_max      14.48

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1008
_exptl_absorpt_coefficient_mu    0.160
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.9534
_exptl_absorpt_correction_T_max  0.9610
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17145
_diffrn_reflns_av_R_equivalents  0.1163
_diffrn_reflns_av_sigmaI/netI    0.1204
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.80
_diffrn_reflns_theta_max         24.99
_reflns_number_total             4297
_reflns_number_gt                1780
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0323P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0034(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4297
_refine_ls_number_parameters     326
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1723
_refine_ls_R_factor_gt           0.0540
_refine_ls_wR_factor_ref         0.1116
_refine_ls_wR_factor_gt          0.0888
_refine_ls_goodness_of_fit_ref   0.900
_refine_ls_restrained_S_all      0.900
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C -0.1980(4) 0.0708(2) 0.12032(17) 0.0485(9) Uani 1 1 d . . .
C2 C -0.2620(4) 0.1562(2) 0.13876(17) 0.0585(10) Uani 1 1 d . . .
H2 H -0.2045 0.2049 0.1578 0.070 Uiso 1 1 calc R . .
C3 C -0.4110(4) 0.1689(3) 0.12888(18) 0.0662(11) Uani 1 1 d . . .
H3 H -0.4532 0.2264 0.1410 0.079 Uiso 1 1 calc R . .
C4 C -0.4978(4) 0.0971(3) 0.1013(2) 0.0747(12) Uani 1 1 d . . .
H4 H -0.5980 0.1060 0.0942 0.090 Uiso 1 1 calc R . .
C5 C -0.4347(4) 0.0125(3) 0.08432(18) 0.0662(11) Uani 1 1 d . . .
H5 H -0.4933 -0.0368 0.0671 0.079 Uiso 1 1 calc R . .
C6 C -0.2855(4) -0.0011(2) 0.09227(17) 0.0543(9) Uani 1 1 d . . .
H6 H -0.2440 -0.0583 0.0789 0.065 Uiso 1 1 calc R . .
C7 C 0.0237(4) -0.0310(2) 0.13268(19) 0.0530(10) Uani 1 1 d . . .
C8 C -0.0233(4) -0.0991(3) 0.17891(19) 0.0668(11) Uani 1 1 d . . .
H8 H -0.0994 -0.0856 0.2086 0.080 Uiso 1 1 calc R . .
C9 C 0.0425(5) -0.1872(3) 0.1811(2) 0.0746(12) Uani 1 1 d . . .
H9 H 0.0092 -0.2334 0.2117 0.090 Uiso 1 1 calc R . .
C10 C 0.1575(5) -0.2074(3) 0.1383(3) 0.0852(14) Uani 1 1 d . . .
H10 H 0.2026 -0.2665 0.1405 0.102 Uiso 1 1 calc R . .
C11 C 0.2042(4) -0.1405(3) 0.0930(2) 0.0816(13) Uani 1 1 d . . .
H11 H 0.2811 -0.1543 0.0639 0.098 Uiso 1 1 calc R . .
C12 C 0.1393(4) -0.0521(3) 0.0894(2) 0.0659(11) Uani 1 1 d . . .
H12 H 0.1727 -0.0068 0.0582 0.079 Uiso 1 1 calc R . .
C13 C 0.0464(4) 0.1411(2) 0.12667(18) 0.0530(9) Uani 1 1 d . . .
C14 C 0.1375(4) 0.1762(2) 0.17787(19) 0.0567(10) Uani 1 1 d . . .
H14 H 0.1523 0.1478 0.2218 0.068 Uiso 1 1 calc R . .
C15 C 0.2078(4) 0.2606(2) 0.15756(19) 0.0566(10) Uani 1 1 d . . .
H15 H 0.2744 0.2930 0.1868 0.068 Uiso 1 1 calc R . .
C16 C 0.1691(3) 0.2900(2) 0.09140(18) 0.0483(9) Uani 1 1 d . . .
C17 C 0.1879(3) 0.4852(2) -0.04281(18) 0.0455(9) Uani 1 1 d . . .
C18 C 0.1496(3) 0.4017(2) -0.01026(18) 0.0495(9) Uani 1 1 d . . .
H18 H 0.0825 0.3611 -0.0326 0.059 Uiso 1 1 calc R . .
C19 C 0.2099(3) 0.3775(2) 0.05531(18) 0.0471(9) Uani 1 1 d . . .
C20 C 0.3104(3) 0.4410(2) 0.08602(17) 0.0503(9) Uani 1 1 d . . .
H20 H 0.3556 0.4274 0.1295 0.060 Uiso 1 1 calc R . .
C21 C 0.3422(3) 0.5242(2) 0.05146(18) 0.0446(9) Uani 1 1 d . . .
C22 C 0.1898(4) 0.5873(3) -0.1497(2) 0.0756(12) Uani 1 1 d . . .
H22 H 0.2692 0.6183 -0.1281 0.091 Uiso 1 1 calc R . .
C23 C 0.1283(4) 0.5134(2) -0.11354(18) 0.0508(9) Uani 1 1 d . . .
C24 C 0.0110(4) 0.4682(3) -0.1461(2) 0.0719(12) Uani 1 1 d . . .
H24 H -0.0337 0.4173 -0.1243 0.086 Uiso 1 1 calc R . .
C25 C -0.0397(5) 0.4999(3) -0.2118(2) 0.0851(13) Uani 1 1 d . . .
H25 H -0.1196 0.4707 -0.2344 0.102 Uiso 1 1 calc R . .
C26 C 0.0285(5) 0.5739(3) -0.2427(2) 0.0841(13) Uani 1 1 d . . .
H26 H -0.0072 0.5948 -0.2865 0.101 Uiso 1 1 calc R . .
C27 C 0.5975(4) 0.6396(3) 0.1771(2) 0.0836(13) Uani 1 1 d . . .
H27 H 0.6365 0.6281 0.2222 0.100 Uiso 1 1 calc R . .
C28 C 0.6385(4) 0.7208(3) 0.1432(3) 0.0816(14) Uani 1 1 d . . .
H28 H 0.7041 0.7628 0.1650 0.098 Uiso 1 1 calc R . .
C29 C 0.5822(4) 0.7394(3) 0.0774(3) 0.0747(12) Uani 1 1 d . . .
H29 H 0.6092 0.7937 0.0533 0.090 Uiso 1 1 calc R . .
C30 C 0.4842(4) 0.6758(2) 0.04718(19) 0.0598(10) Uani 1 1 d . . .
H30 H 0.4431 0.6875 0.0025 0.072 Uiso 1 1 calc R . .
C31 C 0.4467(3) 0.5943(2) 0.0834(2) 0.0516(9) Uani 1 1 d . . .
N1 N -0.0433(3) 0.05984(19) 0.12895(15) 0.0597(8) Uani 1 1 d . . .
N2 N 0.2829(3) 0.54733(17) -0.01204(14) 0.0491(7) Uani 1 1 d . . .
N3 N 0.5033(3) 0.5755(2) 0.14818(16) 0.0729(9) Uani 1 1 d . . .
N4 N 0.1442(4) 0.6180(2) -0.21331(19) 0.0926(11) Uani 1 1 d . . .
S1 S 0.04865(11) 0.21058(6) 0.05139(5) 0.0655(3) Uani 1 1 d . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C6 1.387(4) . ?
C1 C2 1.389(4) . ?
C1 N1 1.427(4) . ?
C2 C3 1.381(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.378(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.368(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.381(4) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 C8 1.379(4) . ?
C7 C12 1.393(4) . ?
C7 N1 1.420(4) . ?
C8 C9 1.381(4) . ?
C8 H8 0.9300 . ?
C9 C10 1.381(5) . ?
C9 H9 0.9300 . ?
C10 C11 1.355(5) . ?
C10 H10 0.9300 . ?
C11 C12 1.381(5) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C14 1.352(4) . ?
C13 N1 1.410(4) . ?
C13 S1 1.732(3) . ?
C14 C15 1.412(4) . ?
C14 H14 0.9300 . ?
C15 C16 1.357(4) . ?
C15 H15 0.9300 . ?
C16 C19 1.464(4) . ?
C16 S1 1.728(3) . ?
C17 N2 1.351(3) . ?
C17 C18 1.381(4) . ?
C17 C23 1.485(4) . ?
C18 C19 1.386(4) . ?
C18 H18 0.9300 . ?
C19 C20 1.397(4) . ?
C20 C21 1.379(4) . ?
C20 H20 0.9300 . ?
C21 N2 1.344(4) . ?
C21 C31 1.490(4) . ?
C22 N4 1.335(4) . ?
C22 C23 1.378(4) . ?
C22 H22 0.9300 . ?
C23 C24 1.376(4) . ?
C24 C25 1.388(5) . ?
C24 H24 0.9300 . ?
C25 C26 1.359(5) . ?
C25 H25 0.9300 . ?
C26 N4 1.332(5) . ?
C26 H26 0.9300 . ?
C27 N3 1.352(4) . ?
C27 C28 1.372(5) . ?
C27 H27 0.9300 . ?
C28 C29 1.358(5) . ?
C28 H28 0.9300 . ?
C29 C30 1.379(4) . ?
C29 H29 0.9300 . ?
C30 C31 1.387(4) . ?
C30 H30 0.9300 . ?
C31 N3 1.343(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C6 C1 C2 119.2(3) . . ?
C6 C1 N1 121.5(3) . . ?
C2 C1 N1 119.3(3) . . ?
C3 C2 C1 120.0(3) . . ?
C3 C2 H2 120.0 . . ?
C1 C2 H2 120.0 . . ?
C4 C3 C2 120.6(4) . . ?
C4 C3 H3 119.7 . . ?
C2 C3 H3 119.7 . . ?
C5 C4 C3 119.1(4) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
C4 C5 C6 121.3(4) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 H5 119.4 . . ?
C5 C6 C1 119.7(3) . . ?
C5 C6 H6 120.1 . . ?
C1 C6 H6 120.1 . . ?
C8 C7 C12 119.0(3) . . ?
C8 C7 N1 121.0(4) . . ?
C12 C7 N1 119.9(3) . . ?
C9 C8 C7 120.0(4) . . ?
C9 C8 H8 120.0 . . ?
C7 C8 H8 120.0 . . ?
C10 C9 C8 120.5(4) . . ?
C10 C9 H9 119.7 . . ?
C8 C9 H9 119.7 . . ?
C11 C10 C9 119.5(4) . . ?
C11 C10 H10 120.2 . . ?
C9 C10 H10 120.2 . . ?
C10 C11 C12 121.0(4) . . ?
C10 C11 H11 119.5 . . ?
C12 C11 H11 119.5 . . ?
C11 C12 C7 119.9(4) . . ?
C11 C12 H12 120.1 . . ?
C7 C12 H12 120.1 . . ?
C14 C13 N1 128.3(3) . . ?
C14 C13 S1 111.2(3) . . ?
N1 C13 S1 120.5(3) . . ?
C13 C14 C15 112.8(3) . . ?
C13 C14 H14 123.6 . . ?
C15 C14 H14 123.6 . . ?
C16 C15 C14 113.8(3) . . ?
C16 C15 H15 123.1 . . ?
C14 C15 H15 123.1 . . ?
C15 C16 C19 128.9(3) . . ?
C15 C16 S1 110.5(2) . . ?
C19 C16 S1 120.6(3) . . ?
N2 C17 C18 121.9(3) . . ?
N2 C17 C23 115.3(3) . . ?
C18 C17 C23 122.8(3) . . ?
C17 C18 C19 120.8(3) . . ?
C17 C18 H18 119.6 . . ?
C19 C18 H18 119.6 . . ?
C18 C19 C20 116.9(3) . . ?
C18 C19 C16 121.8(3) . . ?
C20 C19 C16 121.3(3) . . ?
C21 C20 C19 119.6(3) . . ?
C21 C20 H20 120.2 . . ?
C19 C20 H20 120.2 . . ?
N2 C21 C20 123.2(3) . . ?
N2 C21 C31 115.9(3) . . ?
C20 C21 C31 120.9(3) . . ?
N4 C22 C23 125.1(4) . . ?
N4 C22 H22 117.5 . . ?
C23 C22 H22 117.5 . . ?
C24 C23 C22 116.9(4) . . ?
C24 C23 C17 122.5(3) . . ?
C22 C23 C17 120.6(3) . . ?
C23 C24 C25 119.0(4) . . ?
C23 C24 H24 120.5 . . ?
C25 C24 H24 120.5 . . ?
C26 C25 C24 119.3(4) . . ?
C26 C25 H25 120.3 . . ?
C24 C25 H25 120.3 . . ?
N4 C26 C25 123.2(4) . . ?
N4 C26 H26 118.4 . . ?
C25 C26 H26 118.4 . . ?
N3 C27 C28 123.3(4) . . ?
N3 C27 H27 118.4 . . ?
C28 C27 H27 118.4 . . ?
C29 C28 C27 119.3(4) . . ?
C29 C28 H28 120.3 . . ?
C27 C28 H28 120.3 . . ?
C28 C29 C30 118.5(4) . . ?
C28 C29 H29 120.7 . . ?
C30 C29 H29 120.7 . . ?
C29 C30 C31 120.0(4) . . ?
C29 C30 H30 120.0 . . ?
C31 C30 H30 120.0 . . ?
N3 C31 C30 121.5(3) . . ?
N3 C31 C21 117.5(3) . . ?
C30 C31 C21 120.9(3) . . ?
C13 N1 C7 118.9(3) . . ?
C13 N1 C1 119.0(3) . . ?
C7 N1 C1 121.9(3) . . ?
C21 N2 C17 117.6(3) . . ?
C31 N3 C27 117.3(3) . . ?
C26 N4 C22 116.5(4) . . ?
C16 S1 C13 91.70(17) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 -0.2(5) . . . . ?
N1 C1 C2 C3 178.2(3) . . . . ?
C1 C2 C3 C4 0.5(5) . . . . ?
C2 C3 C4 C5 0.6(6) . . . . ?
C3 C4 C5 C6 -2.1(6) . . . . ?
C4 C5 C6 C1 2.4(5) . . . . ?
C2 C1 C6 C5 -1.2(5) . . . . ?
N1 C1 C6 C5 -179.5(3) . . . . ?
C12 C7 C8 C9 -0.9(5) . . . . ?
N1 C7 C8 C9 179.3(3) . . . . ?
C7 C8 C9 C10 1.3(5) . . . . ?
C8 C9 C10 C11 -1.1(6) . . . . ?
C9 C10 C11 C12 0.5(6) . . . . ?
C10 C11 C12 C7 -0.2(6) . . . . ?
C8 C7 C12 C11 0.4(5) . . . . ?
N1 C7 C12 C11 -179.9(3) . . . . ?
N1 C13 C14 C15 -178.5(3) . . . . ?
S1 C13 C14 C15 1.3(4) . . . . ?
C13 C14 C15 C16 0.6(4) . . . . ?
C14 C15 C16 C19 174.4(3) . . . . ?
C14 C15 C16 S1 -2.2(4) . . . . ?
N2 C17 C18 C19 -1.2(5) . . . . ?
C23 C17 C18 C19 178.9(3) . . . . ?
C17 C18 C19 C20 -0.3(5) . . . . ?
C17 C18 C19 C16 179.0(3) . . . . ?
C15 C16 C19 C18 -173.6(3) . . . . ?
S1 C16 C19 C18 2.7(4) . . . . ?
C15 C16 C19 C20 5.6(5) . . . . ?
S1 C16 C19 C20 -178.1(2) . . . . ?
C18 C19 C20 C21 1.5(4) . . . . ?
C16 C19 C20 C21 -177.8(3) . . . . ?
C19 C20 C21 N2 -1.3(5) . . . . ?
C19 C20 C21 C31 178.8(3) . . . . ?
N4 C22 C23 C24 0.0(6) . . . . ?
N4 C22 C23 C17 -180.0(3) . . . . ?
N2 C17 C23 C24 -167.3(3) . . . . ?
C18 C17 C23 C24 12.6(5) . . . . ?
N2 C17 C23 C22 12.7(5) . . . . ?
C18 C17 C23 C22 -167.4(3) . . . . ?
C22 C23 C24 C25 -1.0(5) . . . . ?
C17 C23 C24 C25 179.0(3) . . . . ?
C23 C24 C25 C26 0.7(6) . . . . ?
C24 C25 C26 N4 0.7(7) . . . . ?
N3 C27 C28 C29 0.4(6) . . . . ?
C27 C28 C29 C30 0.6(6) . . . . ?
C28 C29 C30 C31 -1.0(5) . . . . ?
C29 C30 C31 N3 0.4(5) . . . . ?
C29 C30 C31 C21 -179.4(3) . . . . ?
N2 C21 C31 N3 177.2(3) . . . . ?
C20 C21 C31 N3 -2.9(4) . . . . ?
N2 C21 C31 C30 -3.0(4) . . . . ?
C20 C21 C31 C30 176.8(3) . . . . ?
C14 C13 N1 C7 -67.8(5) . . . . ?
S1 C13 N1 C7 112.5(3) . . . . ?
C14 C13 N1 C1 118.4(4) . . . . ?
S1 C13 N1 C1 -61.3(4) . . . . ?
C8 C7 N1 C13 135.0(3) . . . . ?
C12 C7 N1 C13 -44.7(4) . . . . ?
C8 C7 N1 C1 -51.4(5) . . . . ?
C12 C7 N1 C1 128.9(3) . . . . ?
C6 C1 N1 C13 151.9(3) . . . . ?
C2 C1 N1 C13 -26.5(4) . . . . ?
C6 C1 N1 C7 -21.7(5) . . . . ?
C2 C1 N1 C7 159.9(3) . . . . ?
C20 C21 N2 C17 -0.1(4) . . . . ?
C31 C21 N2 C17 179.7(3) . . . . ?
C18 C17 N2 C21 1.4(4) . . . . ?
C23 C17 N2 C21 -178.7(3) . . . . ?
C30 C31 N3 C27 0.6(5) . . . . ?
C21 C31 N3 C27 -179.7(3) . . . . ?
C28 C27 N3 C31 -1.0(6) . . . . ?
C25 C26 N4 C22 -1.6(6) . . . . ?
C23 C22 N4 C26 1.3(6) . . . . ?
C15 C16 S1 C13 2.4(3) . . . . ?
C19 C16 S1 C13 -174.5(3) . . . . ?
C14 C13 S1 C16 -2.1(3) . . . . ?
N1 C13 S1 C16 177.7(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.212
_refine_diff_density_min         -0.176
_refine_diff_density_rms         0.047
